Preparation of cellulose



Patented June 12, 1928.

y UNITED STATES! PATENT OFFICE.

PRQSPER EAN AUGUSIE MAIGN EN, 01 PHILADELPHIA, PENNSYLVANIA.

PREPARATION No Drawing.

My invention relates to. the preparation of cellulose from fibrous vegetable matter.

The fibrous tissues of plants from which paper, paperboard, celluloid, smokeless powder, viscose, textile fibers, and various other commodities are made or can be made, consist of a skeleton, structure of fibers and cells, generally known as cellulose, and of vari ous ingredients or compounds known generally as non-cellulose or lignone and variously termed impurities, soluble derivatives, fatty and waxy bodies, gums andresins, organic compounds, extractive matter, incrusting materials, etc.

To render plant-tissues available for mak- .ing paper,straw board, wood'board, etc, and for certain other purposes, it is neces sary to dissociate or separate the non-Celialose from thecellulose. I l

1n the preparation of plant-tissues for the above purposes, various processes-are used which are not altogether satisfactory. Thus, for instance, when straw is treated with lime, the .incrusting material is not suiiiciently separated from the cellulose, particularly in theknots, and the, resulting fiber is comparatively hard and brittle. .When flax straw and esparto grass are treated with caustic soda, the fibers are liable to be gela-.

tinized.

Such processes of the prior art are carried on in containers known as rotaries, digesters, or cookers. The aqueous alkaline solution and the material to be treated are introduced in the cooker; high pressure steam turned on, and cooking begins.

WVhen the material to be treated is of the nature of straw or grass which is bulky, it cannot be introduced all at once. Therefore, it has to be put in the cooker in separatebatches. If the aqueous alkaline solution' he made with caustic soda, the first batch is more highly digested than the successive batches. The problem of even diges' or CELLULOSE.

Application filed July 2, 1924. Serial No. 723,686.

tion for these two different kinds of constituents, as is the ordinary practice.

I obtain the desirable degree of alkalinity for these two different classes of non-cellulose ingredients by progressively preparing the alkaline reagent,sodium hydroxide, in the cooker; instead of buying it ready-made on the market, or making it at the mill, before placing it in the cooker, which requires a special causticizing apparatus.

For instance, I find it convenient to mix the reagents to make the sodium hydroxide in the cooker, by first mixing and preferably sieving together, in dry powdered form, calcium hydrate (Water slacked lime) and sodium carbonate (soda ash). I then make a dense colloidal emulsion from said dry mixed chemicals by introducing them into a small quantity of hot Water, but sufficient to enable the mixture to flow into a larger volume or stream of cold water on its wa y to the cooker. Of course, the cold water restrains the reactionary tendencies of said mixture, and such restraining action is enhanced by the low temperature of the material with which the diluted emulsion comes in contact in the cooker. However. when heat is applied, the rezmtionary tendencies oi' the mixture are gradually released from such restraint and reaction progresses in proportion to the amount of heat and the time during which it is applied. That is to say; the reagent sodium hydroxide is thus progressively formed in the cooker by the progressive reaction of calcium hydrate and sodium carbonate, until the nulximum quantity producible by such reaction is formed. Consequcntl y, the sodium hydroxide strength of the solution in the cooker thus gradually increased, by such. reaction until the maximum efl'ect thereof is attained and. thereafter, the strength increases as the sol u tion is concentrated by the boiling oil of the Water vapor from said solutionot sodium hydroxide in the cooker.

The preparation of the alkaline reagent in the cooker saves overhead charges and sundry other expenses, as compared with the use of the previously-made reagent.

The preparing ot the reagent, sodium hydroxide, in the cooker provides a weak alkaline solution for the hydrolyzation of the more readily hydrolyzable constituents at the beginning of the cooking operation and a stronger solution for the hydrolyzation of the less readily hydrolyzable constituents as the oki g ex r on eed F rt ername, the action of the nascent and progresslvely developed reagent, sodium hydroxide,

s effectiye in producin he sepa tion of 'n'iQi-e or less delicate plant-tissues, such as grasses, straw and the like- Eor the treatment of the harder plantw tissue-a as ground Wood, I prefer to use cans tic soda andcaustic lime together, to make in the c oke t e. product known as sqdillime. a

L how e may-use th one .1 th ot r for all k nd of P HH Tt TSU SY- The chemicals used to make the reagent in the a kera e pre erab y mixed in ubstana ly equalspa ts utmay be ixed in any desired Proportion, and app i d in a y 19- sired quantity, according tothe nature of the plant-t ss e to be tr a e an a o d ng to the perio o ookin l i1 9l= a a My pwce m y be c rrie onwith he m n r rer-m l quipmentfin a ines, indrical d eesters, o a y ether lo e ooker with steam press r o it may e ef fe fi d n Qiien anks heated it st am p pe r. ive t am- Among t e ad aImag s "o my in tion are thefollowing: r

The net cost oli the chemicals used to make thereagent, sodium hyclro xi de, the oblin},-

is aln ostnegligg'gible, because no great expense is entailed in the preparation and, more particularly. because the lime and the oda ha fert iz ng v ve Whifi *U W- coyered for the greater part in combination or miXGQl with the organic and norganic constituents of the non-cellulose solute.

Such s lu e by-p 'cdu my f m n aian fa utgu'e o Pap plant t me as bl V as f? m ml flrli if seen the following analysis 0 m y b the treatment of straw Per cent. Moisturen 45.49 Nitrogen (calculated as NH 0.86 Phosphoric acid (calculated as E0 0.14 Potash (calcu at d as K 0) (1.85. Sodium (calculated as figla Q); .Q; "t. 5 C cium canned mi -74;;- 1x

Ot er ing dl nts, in fi'ing' A i's,

reams ex e ugar etevmimiei, s ame 46-3 to the precise details of irocedni'efherein set forth, as is obvious that varions rnodiflpations naybe made therein withcxnt"depart ing froin the essential features of my :ine t n; a de i eat the e 'l i g Wm I claim q q w-id has a wander; v

' a: semifluid sample of such spl n pgspltiqg from.

f myself A m od "o treati g B ah? fis i e? 1 eckei' or. the P rpose of S parati g h cellulose from the non-cellulose constituents thereof withoutinrairment 'o the value qf I h tt r fo play ert lir e P 1 B b subjecting raw material to e p 0 ressive gressively generated in the cooker 1r m x ure bf s bst ntiall q u m 01 1" dinrn carbonate and calcmm hydrate in water, while maintaining the mass at qtrnospheric pressure; the reaction of said h mical b mg rog issi a wm a n thepresence of s cl 1"tiss1 1 es|; and separating the non-cellulose oonstitiients from the'cell ilose with said chemicals and the rflsidues' ofthe reaction thereof; the soltltion is us removed being characterized by beneficial action upon plants, and cellulose thus treated being in condition for use in te I test mony whereof, 'I have hereunto signed my name at Philadelphia, Pennsylmm, this thirtieth day of June, 19%

" P1105752 JEN! comm: u. 

